Brown sulfur dye.



UNITED STATES PATENT ALFRED HERRE AND BERNiIARD JAECKEL, OF ELBERFIILD, GERVAN Y, ASSIGNORS 'I O FA BENFABRIKEN VORM. FRIEDR. 'IION 0F GERMANY.

BROWN SULFURDYE.

Specification of Letters Patent.

Patented sag. 11, 1903.-

Application filed April 8,1908. Serial No. 425,8

To all whom it may concern:

Be it known that we, ALFRED HERRE and BERNHA'RD JAECKEL, doctors of hilosophy, chemists, citizens of the German mpire, residing at Elberfeld, Germany, Kingdom of Prussia, have invented new and useful Improvements in New Brown Sulfur Dyes, of which the following is a specification.

Our invention relates to the manufacture and production of new yellowish-brown to orange sulfur dyestuffs which can be obtained by heating with sulfur mixtures of meta diamins alkylated in the aromatic nucleus with nitroamins or derivatives thereof and transforming the sulfid colors into soluble compounds by heating them with alkaline sullids.

The new est-riffs are after being dried and pulverized dark powders )ractically insoluble in pure water, but soluble in Water in the )resence of sodium sulfid with a brown color, hardly soluble in dilute caustic'soda lye and in concentrated sulfuric acid with a brown color. 4

In order to illustrate the new process more fully the following exan'iple is given, the parts being by weight: 108 parts of meta-toluylenediamin, together with parts of meta-nitranilin and 600 parts of sulfur, are heated to 240%250" C. for 12 hours. \Vhen cold the melt is pulverized and is heated to from -400" C. with 450 parts of a 100 per cent. solution of sodium sulfid and 2000 parts of water until a clear solution resuits. The mixture is then diluted with water and the dyestuff is precipitated with dilute acids. ground.

Our new dyestull' is after being dried and pulverized a dark brown powder which is practically insoluble in pure water, but soluble in water in the presence of sodium sulfid with a brown color, it is hardly soluble in dilutoeaustic soda lye with a brown color and in concentrated sulfuric acid (66 Baum) with a yellowish-brown color. It dyes unmordanted cotton in a bath of sodium sulfid reddish yellmr-brown shades.

The process is carried out in an analogous manner on using other of the above mentioned mixtures.

The same dyestufl's can be obtained by replacing the nitroamino-compounds by the corresponding dinitro compounds or by It is filtered off, dried and heatirfg with sulfur n'iixtu'res of Ineta diamins 0r triamins (derived from Inetai-diamins) or their derivatives with l'iitrimminsjalkylated in the aromatic nucleus or with the respective olynitro connioui'ids and transforming the sulfid colors thus'produc'ed into soluble compounds by heating thenrwithhlkaline sulfids. a p

In the followingtnhje the shadeaof'some of'the. new dyestuffs are givh:

Dyestull obtained from: Dyes cotton:

(1) Meta; toluylenedhunln +n1etai- *Reqdlsh'yellnw-brown. nitmnilin (2) Metie toluyleuedlumin paraam (3) IlIem-toluylenedmmln 4-1Xltl'0' Iladdishqellow-browh.

(4) Mcta-tnluylenedlamln dlnitm- Orange.

dineetbenzldln (5) Metmtohiylenedinmln dlnltrm Orange.

dihenzoylhenzhlin- (G) Meta-tolliylenedlmnin lomiyl- Yellow-brown.

lteddlsh yellow-brown. Yellow-brown. Reddlah yellow-brown. Reqdlsh yellow-bro wn.

Yellowish-hrown. Yellom'bmivn. Yellowsbmwn. Brownian-yellow. Orange-yellow. Yellow-brown.

Reuomh yellow-brown. i

Having thus described our invention and in what manner the same is performed, what we'elaim as new, and desire to secure by Let ters Patent, is

1.- The herein-described new sulfur dyestufl's resulting from the reaction of sulfur on a mixture of aromatic nieta-diainins and nitro-nmiiis the one of which izoxnp:;1 rents must he alkvlated in the aromatic nucleus, which are after being dried and, )ulverized dark powders practically iusoluhe in pure water but soluble in water in the )resence of sodium sulfid with a brown eo or hardly soluble in dilute caustic soda lye and nit-on.-

centrated sulfuric acid with a brown color;

and which dye unmordnnted rot-ton in a bath containing sodium sulfid from yellowish brown'to orange shades, suhsnmtially as hereinbefore described. I

2. The hereiindescriluul new sulfur dyestull resulting from the reaction of sulfur on.

a mixture of meta toluylenedia-min with brown shades, substantially as hereinbcfor" meta-mti'anlhn, inch 1s after bcmg d'flfid described. and pulvcmzegl a dark biown paw 1ns01 in te-s'ilmony whereof W8 have hereunto 11 018111 pure Wat-c1 but Soluble 1'11 Water 111 the se't 0111 hands" in the presence of two su bscribresence 0f sodlum sulfid qt-h a brown color, 111g Witnesses.

11 containing sodium sulfid reddish gw-LOW ardly soluble in dilute caustic soda lye with ALFRED HERRE. [L 3.] HmbI'OXVIl 00101 and soluble in concentrated BERNHARD JAECKEL. [1 3.} sulfuric acid With a yellowish-brown cclor, fl/"imnesscsz "11d which dyes unmcrdanted cotton. in a I ()TTO KQNIG,

WM. WASHINGTQN BRUNSWlOK. 

